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Preparation method of 4-benzyloxy phenyl ethyl n-decanoate

A technology of n-decanoate and benzyloxybenzene, applied in the field of preparation of 4-benzyloxyphenylethyl n-decanoate, can solve the problems of many by-products, long reaction route, easy passivation, etc. The effect of improving production efficiency, simplifying production process and avoiding pollution

Pending Publication Date: 2022-03-22
郑州睿嘉纳米新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 4-Benzyloxyphenylethyl n-decanoate is a thermochromic additive, which is usually obtained by reacting 4-benzyloxyphenylethyl alcohol with n-decanoyl chloride, but the reaction is very slow, and it is easy to blunt after a certain degree of reaction. Therefore, it needs to be improved. There are few reports on the direct esterification of 4-benzyloxyphenylethanol and n-decanoic acid under acid catalysis, but 4-benzyloxyphenylethanol is easy under the condition of higher temperature under acid catalysis. Dehydration causes side reactions to occur, resulting in reduced yield and impure product. The existing 4-benzyloxyphenylethyl n-decanoate preparation process has a long reaction route, cumbersome methods, and many by-products, resulting in low product yield. , poor production efficiency and other issues

Method used

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  • Preparation method of 4-benzyloxy phenyl ethyl n-decanoate
  • Preparation method of 4-benzyloxy phenyl ethyl n-decanoate
  • Preparation method of 4-benzyloxy phenyl ethyl n-decanoate

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Embodiment Construction

[0021] The present invention is described in further detail below in conjunction with embodiment.

[0022] A kind of preparation method of 4-benzyloxyphenylethyl n-decanoate disclosed by the invention comprises the following steps:

[0023] A. Add methanol, p-hydroxyphenethyl alcohol and equivalent benzyl chloride into a clean three-necked flask, stir and mix evenly, then add solid sodium hydroxide in three batches, heat up to reflux after each addition and react for 0.5 hours, Then cool down to 50 degrees and add the next batch of sodium hydroxide, the reaction equation is as follows:

[0024]

[0025] B. After the step A reaction is completed, the solvent is directly distilled out, and then after the solvent is completely distilled, the equivalent of n-decanoyl chloride is directly added dropwise, and the temperature is controlled below 20 degrees. The reaction equation is as follows:

[0026]

[0027] C. After step B is reacted for 1 hour, a large amount of water is ...

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Abstract

The invention discloses a preparation method of 4-benzyloxy phenyl ethyl n-decanoate, which comprises the following steps: A, adding methanol, p-hydroxyphenethyl alcohol and equivalent benzyl chloride into a clean three-neck flask, uniformly stirring and mixing, then adding sodium hydroxide solid in three batches, heating to reflux after each time of addition, and reacting for 0.5 hour, so as to obtain 4-benzyloxy phenyl ethyl n-decanoate; b, after the reaction is finished, directly distilling out the solvent, then after the solvent is completely distilled, directly dropwise adding n-decanoyl chloride with the same equivalent amount, and controlling the temperature to be lower than 20 DEG C, C, after the reaction is finished, adding a large amount of water, separating out a large amount of product at the moment, uniformly stirring, and centrifuging to obtain a crude product; and D, adding ethanol into the crude product, heating and dissolving, cooling and separating out, and centrifuging again to obtain a refined product 4-benzyloxy phenyl ethyl n-decanoate. In the reaction stage, the usage amount of solvents and reagents is reduced, no acid-binding agent is used, and therefore pollution to the environment is reduced, no by-product exists in the reaction process, and the production process is more environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of biochemical industry, in particular to a preparation method of 4-benzyloxyphenylethyl n-decanoate. Background technique [0002] 4-Benzyloxyphenylethyl n-decanoate is a thermochromic additive, which is usually obtained by reacting 4-benzyloxyphenylethyl alcohol with n-decanoyl chloride, but the reaction is very slow, and it is easy to blunt after a certain degree of reaction. Therefore, it needs to be improved. There are few reports on the direct esterification of 4-benzyloxyphenylethanol and n-decanoic acid under acid catalysis, but 4-benzyloxyphenylethanol is easy under the condition of higher temperature under acid catalysis. Dehydration causes side reactions, resulting in reduced yield and impure product. The existing 4-benzyloxyphenylethyl n-decanoate preparation process has a long reaction route, cumbersome methods, and many by-products, resulting in low product yield. , Poor production efficiency ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/14C07C41/16C07C67/52C07C67/48C07C69/28C07C43/253
CPCC07C67/14C07C41/16C07C67/52C07C67/48C07C69/28C07C43/253
Inventor 耿定金杨会会陈通宋广寒
Owner 郑州睿嘉纳米新材料科技有限公司
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